CN112680965A

CN112680965A - Water-dispersible composition for fiber processing

Info

Publication number: CN112680965A
Application number: CN202011109895.4A
Authority: CN
Inventors: 小川寿子
Original assignee: Arakawa Chemical Industries Ltd
Current assignee: Arakawa Chemical Industries Ltd
Priority date: 2019-10-17
Filing date: 2020-10-16
Publication date: 2021-04-20
Also published as: JP2021066990A; JP7435400B2; TW202124664A

Abstract

The invention provides a water-dispersible composition for fiber processing, which can obtain a fiber product with excellent slipping property, hand feeling and chalk mark resistance without damaging the functions of fiber processing agents such as water repellency, durable water repellency and antifouling property. The invention provides a water-dispersible composition for fiber processing, which contains a rosin resin as a component (A) and a nonionic surfactant as a component (B).

Description

Water-dispersible composition for fiber processing

Technical Field

The present invention relates to a water-dispersible composition for fiber processing.

Background

Conventionally, fibers are often processed with various fiber processing agents in order to impart various functions such as water repellency and stain resistance to the fibers.

For example, as a method for imparting water repellency to fibers, treatment with a water repellent is generally used. As the water repellent agent, particularly, a fluorine-based water repellent agent having fluorine atoms is widely known, and a fiber product having water repellency imparted to the surface thereof by treating a fiber product or the like with the fluorine-based water repellent agent is known.

The fluorine-based water repellent agent is generally produced by polymerizing or copolymerizing a monomer having a fluoroalkyl group. Fiber products treated with a fluorine-based water repellent exhibit excellent water repellency, but since a monomer having a fluoroalkyl group is hardly decomposed, there is a problem in terms of environment.

Therefore, in recent years, studies have been made on a non-fluorine water repellent containing no fluorine atom. For example, patent document 1 proposes a water repellent agent composed of a specific non-fluorinated polymer containing a (meth) acrylate ester having 12 or more carbon atoms as a monomer unit. Patent document 2 proposes a soft water repellent containing an amino-modified silicone and a polyfunctional isocyanate compound. However, since fibers processed using these water repellent agents have extremely low frictional resistance between fibers, there is a problem that slippage (performance of preventing a seam displacement phenomenon in wearing in clothes and the like) is reduced. Further, the processed fiber tends to be hard, and therefore the hand is not sufficient. Further, when the processed fiber is bent or rubbed, there is a problem that the water repellent coating on the fiber is cracked or peeled off, and the portion is whitened by diffuse reflection of light, so-called chalk marks are generated, and the appearance is largely impaired.

In addition, as another functional property imparted to the fiber, there is a stain-proofing treatment. Conventionally, various methods of antifouling treatment have been proposed in order to prevent stains from adhering to fibers or to facilitate removal of the adhering stains.

As the above-mentioned stain-proofing treatment, for example, non-fluorine-based stain-proofing (SG, Soil Guard; property of making stain components less likely to adhere to the fiber surface) treatment in which the fiber surface is coated with a stain-resistance-imparting agent such as a silicone-based treating agent is known. When the SG processing is performed on the fiber, it becomes difficult for liquid stains to adhere to the fiber surface. However, in such SG processing, since frictional resistance between fibers is reduced, there is a problem that, similarly to the above water repellent processing, slippage of fibers is reduced and the hand feeling thereof is also deteriorated.

Patent document 3 proposes an antifouling agent having excellent SG properties by adhering polysaccharides and modified fine organosilicate particles to a fiber material. However, the slippage of the fiber or its hand is not considered.

Documents of the prior art

Patent document 1: japanese patent laid-open No. 2006-328624.

Patent document 2: japanese patent laid-open No. 2004-059609.

Patent document 3: japanese patent laid-open No. 2014-122435.

Disclosure of Invention

The present invention has been made in view of the above circumstances, and an object thereof is to provide a water-dispersible composition for fiber processing, which can obtain a fiber product excellent in slipperiness, texture and chalk mark resistance without impairing the functions of a fiber processing agent such as water repellency, durable water repellency and stain resistance.

The present inventors have made extensive studies and as a result, have found that the above problems can be solved by using a composition in which a nonionic surfactant for rosin-based resins is dispersed in water. That is, the present invention relates to the following water-dispersible composition for fiber processing.

(1) A water-dispersible composition for fiber processing, which comprises a rosin-based resin as a component (A) and a nonionic surfactant as a component (B).

(2) The water-dispersible composition for fiber processing according to (1), wherein the rosin-based resin as the component (A) has a softening point of 80 to 180 ℃.

(3) The water-dispersible composition for fiber processing according to (1) or (2), wherein the rosin-based resin as the component (A) is a rosin ester.

(4) The water-dispersible composition for fiber processing according to any one of (1) to (3) above, wherein the nonionic surfactant as component (B) has an HLB (Hydrophile lipophile Balance) of 7 to 19.

(5) The water-dispersible composition for fiber processing according to any one of (1) to (4) above, which is used for polyester fibers.

(6) The water-dispersible composition for fiber processing according to any one of (1) to (4) above, wherein the composition is used for polyamide fibers.

(7) The water-dispersible composition for fiber processing according to any one of (1) to (4) above, wherein the composition is used for cotton.

According to the water-dispersible composition for fiber processing of the present invention, when used in combination with a fiber processing agent, a fiber product excellent in slipperiness, hand feeling and chalk mark resistance can be obtained without impairing the functions of the fiber processing agent such as water repellency, durable water repellency and stain resistance. The water-dispersible composition for fiber processing can be applied to various fiber processing agents, but is preferably used as a water repellent agent or a stain resistance-imparting agent. Further, the above-mentioned water-dispersible composition for fiber processing is preferably used for polyester fibers or cotton.

Detailed Description

[ Water-dispersible composition for fiber processing ]

The water-dispersible composition for fiber processing (hereinafter, also simply referred to as "composition") of the present invention contains a rosin resin (a) (hereinafter, referred to as "component (a)") and a nonionic surfactant (B) (hereinafter, referred to as "component (B)").

< rosin-based resin (A) >)

The component (a) is not particularly limited, and various known substances can be used. (A) Examples of the component(s) include natural rosins (gum rosin, tall oil rosin, wood rosin) derived from masson pine, Slash pine (Slash pine), southern pine (Merkus pine), pinus khasys, Loblolly pine (lobelly pine), and Longleaf pine (Longleaf pine); a purified rosin obtained by purifying natural rosin by a vacuum distillation method, a steam distillation method, an extraction method, a recrystallization method, or the like (hereinafter, natural rosin and purified rosin are also referred to as unmodified rosin); hydrogenated rosin obtained by subjecting the unmodified rosin to a hydrogenation reaction; disproportionated rosin obtained by subjecting the unmodified rosin to a disproportionation reaction; a polymerized rosin obtained by polymerizing the unmodified rosin; an α, β -unsaturated carboxylic acid-modified rosin such as an acrylated rosin, a maleated rosin, or a fumarated rosin, an esterified product of these (hereinafter, the esterified product of these is referred to as a rosin ester), a rosin phenol resin, and the like. (A) The components may be used singly or in combination of two or more.

(A) The component (b) is preferably a rosin ester, more preferably at least one selected from the group consisting of an unmodified rosin ester, a hydrogenated rosin ester, a disproportionated rosin ester, a polymerized rosin ester and an α, β -unsaturated carboxylic acid-modified rosin ester, from the viewpoint of excellent fiber slippage, chalk mark resistance, hand feeling and composition stability, and particularly preferably an unmodified rosin ester of hydrogenated rosin ester, a disproportionated rosin ester, an α, β -unsaturated carboxylic acid-modified rosin ester or an unmodified rosin ester of a southern pine-derived unmodified rosin, from the same viewpoint. Hereinafter, unmodified rosin esters, hydrogenated rosin esters, disproportionated rosin esters, polymerized rosin esters, and α, β -unsaturated carboxylic acid-modified rosin esters will be described.

(unmodified rosin ester)

An unmodified rosin ester is obtained by reacting the above unmodified rosin with an alcohol.

As the unmodified rosin, unmodified rosin purified by a vacuum distillation method, a steam distillation method, an extraction method, a recrystallization method, or the like can be used.

The reaction conditions of the unmodified rosin and the alcohol may be about 1 to 8 hours at about 250 to 280 ℃ with or without adding an esterification catalyst as necessary in the presence or absence of a solvent.

The alcohols are not particularly limited, and examples thereof include monohydric alcohols such as methanol, ethanol, propanol, and stearyl alcohol; glycols such as ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, neopentyl glycol, and dimer diol (Dimerdiol); trihydric alcohols such as glycerin, trimethylolethane and trimethylolpropane; tetrahydric alcohols such as pentaerythritol and diglycerin; and hexahydric alcohols such as dipentaerythritol. Among these, polyhydric alcohols having two or more hydroxyl groups are preferable, and in particular, glycerin and pentaerythritol are more preferable.

(hydrogenated rosin ester)

The hydrogenated rosin ester is obtained by esterifying a hydrogenated rosin obtained by hydrogenating the above-mentioned unmodified rosin with an alcohol.

The hydrogenated rosin can be obtained by various known methods. Specifically, for example, the resin can be obtained by hydrogenating the above-mentioned unmodified rosin using a known hydrogenation condition. Examples of the hydrogenation conditions include a method in which the above-mentioned unmodified rosin is heated under a hydrogen pressure of about 2 to 20MPa and at about 100 to 300 ℃ in the presence of a hydrogenation catalyst. Further, it is preferable that the hydrogen pressure is about 5 to 20MPa and the reaction temperature is about 150 to 300 ℃. As the hydrogenation catalyst, various known catalysts such as a supported catalyst and a metal powder can be used. Examples of the supported catalyst include palladium-carbon, rhodium-carbon, ruthenium-carbon, and platinum-carbon. Examples of the metal powder include nickel and platinum. Among these, palladium, rhodium, ruthenium and platinum-based catalysts are preferable because the hydrogenation rate of the unmodified rosin is increased and the hydrogenation time is shortened. The amount of the hydrogenation catalyst to be used is usually about 0.01 to 5 parts by mass, preferably about 0.01 to 2 parts by mass, based on 100 parts by mass of the unmodified rosin.

The hydrogenation may be carried out in a state where the unmodified rosin is dissolved in a solvent, if necessary. The solvent to be used is not particularly limited, and any solvent may be used as long as it is inactive to the reaction and easily dissolves the starting material or product. Specifically, for example, cyclohexane, n-hexane, n-heptane, decalin, tetrahydrofuran, dioxane, etc. can be used alone or in combination of two or more. The amount of the solvent used is not particularly limited, and may be generally in the range of 10 mass% or more, preferably about 10 to 70 mass% of the solid content with respect to the unmodified rosin.

Further, as the hydrogenated rosin, a rosin obtained by subjecting a hydrogenated rosin to the above purification may be used.

The reaction of the hydrogenated rosin and the alcohol may be carried out at about 250 to 280 ℃ for about 1 to 8 hours by adding an esterification catalyst as necessary in the presence or absence of a solvent to the hydrogenated rosin and the alcohol.

The alcohols used in esterifying the hydrogenated rosin are the same as described above.

The order of the hydrogenation reaction and the esterification reaction is not limited to the above, and the hydrogenation reaction may be performed after the esterification reaction.

(disproportionated rosin ester)

The disproportionated rosin ester is obtained by esterifying a disproportionated rosin obtained by disproportionating the above-mentioned unmodified rosin with an alcohol.

The disproportionated rosin can be obtained by various known methods. For example, the above-mentioned unmodified rosin may be heated and reacted in the presence of a disproportionation catalyst. Examples of the disproportionation catalyst include supported catalysts such as palladium-carbon, rhodium-carbon, and platinum-carbon; metal powder such as nickel and platinum; and iodides such as iodine and iron iodide. The amount of the catalyst is usually about 0.01 to 5 parts by mass, preferably about 0.01 to 1 part by mass, per 100 parts by mass of rosin as a raw material, and the reaction temperature is about 100 to 300 ℃ and preferably about 150 to 290 ℃.

Further, as the disproportionated rosin, a rosin obtained by subjecting disproportionated rosin to the above-described purification may be used.

The reaction of the disproportionated rosin and the alcohol may be carried out at about 250 to 280 ℃ for about 1 to 8 hours by adding an esterification catalyst as necessary in the presence or absence of a solvent.

The alcohols used in esterifying the disproportionated rosin are the same as described above.

The order of the disproportionation reaction and the esterification reaction is not limited to the above, and the disproportionation reaction may be performed after the esterification reaction.

(polymerized rosin ester)

The polymerized rosin ester is obtained by reacting a polymerized rosin with an alcohol. Polymerized rosin is a rosin derivative containing dimerized resin acids.

As a method for producing the polymerized rosin, a known method can be employed. Specifically, for example, a method of reacting the above-mentioned unmodified rosin as a raw material in a solvent such as toluene or xylene containing a catalyst such as sulfuric acid, hydrogen fluoride, aluminum chloride, titanium tetrachloride or the like at a temperature of about 40 to 160 ℃ for about 1 to 5 hours, and the like can be mentioned.

Specific examples of the polymerized rosin include a resin-based polymerized rosin using gum rosin as the raw material (for example, a trade name "polymerized rosin B-140", manufactured by newcastle linning limited), a tall oil-based polymerized rosin using tall oil rosin (for example, a trade name "シルバタック 140 (Sylvatac 140)", manufactured by arizona chemical company (アリゾナケミカル)), a wood-based polymerized rosin using wood rosin (for example, a trade name "ダイマレックス (english name: Dymerex)", manufactured by Ashland).

As the polymerized rosin, a polymerized rosin modified by hydrogenation, disproportionation, or the like; or a rosin modified with an α, β -unsaturated carboxylic acid such as an acrylic acid, a maleic acid, or a fumaric acid. Further, each treatment may be used alone or in combination of two or more.

The reaction conditions of the polymerized rosin and the alcohol may be about 1 to 8 hours at about 250 to 280 ℃ with or without a solvent and optionally an esterification catalyst.

The alcohols used in esterifying the polymerized rosin are the same as described above.

The order of the polymerization reaction and the esterification reaction is not limited to the above, and the polymerization reaction may be performed after the esterification reaction.

(alpha, beta-unsaturated Carboxylic acid modified rosin ester)

The α, β -unsaturated carboxylic acid-modified rosin ester is obtained by esterifying a modified rosin obtained by addition reaction of the above-mentioned unmodified rosin or the above-mentioned disproportionated rosin with an α, β -unsaturated carboxylic acid (α, β -unsaturated carboxylic acid-modified rosin) with an alcohol.

The α, β -unsaturated carboxylic acid is not particularly limited, and various known α, β -unsaturated carboxylic acids can be used. Specific examples thereof include acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid, mucofuroic acid, maleic anhydride, itaconic anhydride, citraconic anhydride, and mucofuroic anhydride. Among them, maleic acid, maleic anhydride and fumaric acid are preferable. The amount of the α, β -unsaturated carboxylic acid used is usually about 1 to 20 parts by mass, preferably about 1 to 3 parts by mass, per 100 parts by mass of the unmodified rosin or the disproportionated rosin, from the viewpoint of emulsifiability.

The method for producing the α, β -unsaturated carboxylic acid-modified rosin is not particularly limited, and examples thereof include a method in which the α, β -unsaturated carboxylic acid is added to the unmodified rosin or the disproportionated rosin melted under heating, and the mixture is reacted at a temperature of about 180 to 240 ℃ for about 1 to 9 hours. The reaction may be carried out while blowing an inert gas such as nitrogen into the closed reaction system. In the reaction, for example, a known catalyst such as a lewis acid such as zinc chloride, ferric chloride, or tin chloride, or a bronsted acid such as p-toluenesulfonic acid or methanesulfonic acid may be used. The amount of the catalyst used is usually about 0.01 to 10% by mass based on the unmodified rosin or the disproportionated rosin.

In the obtained α, β -unsaturated carboxylic acid-modified rosin, resin acids derived from the above-mentioned unmodified rosin or the above-mentioned disproportionated rosin may be contained in an amount of less than 10% by mass.

The reaction conditions of the α, β -unsaturated carboxylic acid-modified rosin and the alcohol are not particularly limited, and examples thereof include adding an alcohol to an α, β -unsaturated carboxylic acid-modified rosin melted under heating, and reacting at a temperature of about 250 to 280 ℃ for about 15 to 20 hours. The reaction may be carried out while blowing an inert gas such as nitrogen into the closed reaction system, or the above-mentioned catalyst may be used.

The alcohols used for esterifying the α, β -unsaturated carboxylic acid-modified rosin are the same as described above.

Physical Properties of rosin resin (A)

The physical properties of the component (A) are not particularly limited. (A) The softening point of the component (A) is preferably about 80 to 180 ℃, more preferably about 100 to 140 ℃, and particularly preferably about 120 to 130 ℃ from the viewpoint of excellent fiber hand feeling and composition stability. In the present specification, the softening point is a value measured by the ring and ball method (JIS K5902).

(A) The hydroxyl value of the component (A) is preferably about 10 to 50mgKOH/g from the viewpoint of excellent emulsion stability of the composition. The acid value of the component (A) is preferably about 0.5 to 30mgKOH/g, from the viewpoint of excellent emulsion stability. In the present specification, the hydroxyl value and the acid value are values measured in accordance with JIS K0070.

(A) The weight average molecular weight of the component (a) is preferably about 500 to 3000, more preferably about 1100 to 2000, from the viewpoint of excellent emulsion stability of the composition. In the present specification, the weight average molecular weight is a polystyrene equivalent value obtained by a Gel Permeation Chromatography (GPC) method.

(A) The color tone of the component (A) is preferably not more than 4 Gardner color, more preferably not more than 150 haas, and particularly preferably not more than 60 haas. When the color tone of the component (a) is 4 gardner chroma or less, the fiber product treated with the aqueous dispersion composition for fiber processing of the present invention is inhibited from being colored (yellowed) with time. In addition, when the color tone of the component (a) is harsen grade, the coloring of the fiber product with time is further suppressed. In the present specification, the color tone is measured in Gardner color units and Hamon units according to JIS K0071-3.

< nonionic surfactant (B) >)

The component (B) is not particularly limited as long as it is a nonionic surfactant, and various known nonionic surfactants can be used. In the water-dispersed composition of the present invention, when an anionic surfactant or a cationic surfactant is used instead of the nonionic surfactant (B), various functions (water repellency, stain resistance, etc.) of the fiber-processing agent may be deteriorated or the stability thereof may be deteriorated when the fiber-processing agent is used in combination therewith, which is not preferable. (B) The components may be used singly or in combination of two or more.

(B) Examples of the component (B) include polyoxyethylene alkyl ethers, polyoxyethylene alkenyl ethers, polyoxyethylene alkylphenyl ethers, polyoxypolycyclic phenyl ethers, sorbitan higher fatty acid esters, polyoxyethylene higher fatty acid esters, glycerin higher fatty acid esters, and block copolymers of polyalkylene oxides, and specifically, examples thereof include polyoxyethylene lauryl ether, polyoxyethylene oleyl ether, polyoxyethylene stearyl ether, polyoxyethylene nonylphenyl ether, polyoxyethylene octylphenyl ether, polyoxyethylene styrylphenyl ether, sorbitan monolaurate, sorbitan trioleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene monooleate, oleic acid monoglyceride, stearic acid monoglyceride, and polyoxyethylene-polyoxypropylene block copolymer.

(B) The component (B) is preferably a block copolymer of polyoxyethylene alkyl ether, polyoxyethylene alkenyl ether, sorbitan higher fatty acid ester, polyoxyethylene higher fatty acid ester, glycerin higher fatty acid ester, or polyoxyalkylene.

(physical Properties of nonionic surfactant (B))

The physical properties of the component (B) are not particularly limited. (B) The HLB of component (A) is preferably 7 to 19, and more preferably about 12 to 15, from the viewpoint of excellent emulsion stability of component (A), stability of the fiber processing agent, water repellency, and stain-proofing property. When the HLB of component (B) is 7 or more, the emulsion stability of component (a) and the stability of the fiber processing agent become more excellent. When HLB is 19 or less, the fiber processing agent is more excellent in water repellency and stain resistance. The HLB is a value representing the balance between the hydrophobicity and hydrophilicity of the surfactant, and is a value of 1 to 20, where a smaller value indicates a stronger hydrophobicity, and a larger value indicates a stronger hydrophilicity.

(B) The amount of the component (a) is not particularly limited, but is preferably about 1 to 20 parts by mass, and more preferably about 5 to 10 parts by mass in terms of solid content, based on 100 parts by mass of the component (a). When the amount of the component (B) is 1 part by mass or more, reliable emulsification can be performed, and the stability is improved when the emulsion is used as a water repellent or a stain resistance-imparting agent. Further, when the amount is 20 parts by mass or less, the water repellency is hardly impaired when the composition is used as a water repellent.

< surfactant (C) >

The composition of the present invention may contain a surfactant (C) (hereinafter, also referred to as component (C)) other than component (B) as necessary within a range not impairing the effects of the present invention, for the purpose of improving the dispersibility of the composition.

(C) The component (B) is not particularly limited as long as it is a substance other than the component (a), and various known emulsifiers can be used. Specifically, examples thereof include a high molecular weight emulsifier, a low molecular weight anionic emulsifier, and a low molecular weight cationic emulsifier obtained by polymerizing monomers. These may be used alone or in combination of two or more. Among them, low molecular weight anionic emulsifiers are preferable in terms of excellent emulsifiability.

Examples of the monomer used for producing the high molecular weight emulsifier include (meth) acrylate monomers such as methyl (meth) acrylate and ethyl (meth) acrylate; monocarboxylic acid-based vinyl monomers such as (meth) acrylic acid and crotonic acid; dicarboxylic acid-based vinyl monomers such as maleic acid and maleic anhydride; sulfonic acid vinyl monomers such as vinylsulfonic acid and styrenesulfonic acid; and alkali metal salts, alkaline earth metal salts, ammonium salts, and salts of organic bases of these various organic acids; (meth) acrylamide monomers such as (meth) acrylamide and N-methylol (meth) acrylamide; nitrile monomers such as (meth) acrylonitrile; vinyl ester monomers such as vinyl acetate; hydroxyl group-containing (meth) acrylate monomers such as 2-hydroxyethyl (meth) acrylate and 2-hydroxypropyl (meth) acrylate; methyl vinyl ether, glycidyl (meth) acrylate, urethane acrylate, an α -olefin having 6 to 22 carbon atoms, vinyl pyrrolidone, and other monomers. These may be used alone or in combination of two or more.

Examples of the polymerization method include solution polymerization, suspension polymerization, emulsion polymerization using a reactive emulsifier other than a high-molecular-weight emulsifier, a non-reactive emulsifier other than a high-molecular-weight emulsifier, and the like, which will be described later.

The weight average molecular weight of the high molecular weight emulsifier thus obtained is not particularly limited, but is usually about 1000 to 500000, and the above numerical value is preferable from the viewpoint of the adhesive properties of the resulting tackifier resin emulsion. The weight average molecular weight referred to herein is a polyethylene oxide value obtained by Gel Permeation Chromatography (GPC).

The reactive emulsifier other than the high-molecular-weight emulsifier is, for example, an emulsifier having a hydrophilic group such as a sulfonic acid group or a carboxyl group and a hydrophobic group such as an alkyl group or a phenyl group and having a carbon-carbon double bond in the molecule.

Examples of the low-molecular-weight anionic emulsifier include dialkyl sulfosuccinate salts, alkane sulfonates, α -olefin sulfonates, polyoxyethylene alkyl ether sulfosuccinate salts, polyoxyethylene styryl phenyl ether sulfosuccinate salts, naphthalene sulfonic acid formalin condensates, polyoxyethylene alkyl ether sulfate salts, polyoxyethylene dialkyl ether sulfate salts, polyoxyethylene trialkyl ether sulfate salts, and polyoxyethylene alkyl phenyl ether sulfate salts.

Examples of the low molecular weight cationic emulsifier include tetraalkylammonium chloride, trialkylbenzylammonium chloride, alkylamine acetate, alkylamine hydrochloride, ethyleneoxyalkylamine, polyoxyethylenealkylamine, and alkylamine acetate.

The emulsifiers other than the above high-molecular-weight emulsifiers may be used alone or two or more kinds thereof may be appropriately selected.

(C) The amount of the component (a) is preferably about 1 to 10 parts by mass, more preferably about 2 to 8 parts by mass, per 100 parts by mass of the component (a) in terms of solid content, from the viewpoint of excellent emulsifiability.

The aqueous dispersion composition for fiber processing of the present invention may contain, as necessary, various additives such as a defoaming agent, a thickener, a filler, an antioxidant, a water resistance agent, and a film-forming aid, and a pH adjuster such as ammonia water or sodium hydrogen carbonate, within a range not to impair the desired properties.

[ Process for producing Water-dispersible composition for fiber processing ]

The water-dispersible composition for fiber processing of the present invention is obtained by emulsifying component (a) in water in the presence of component (B) and, if necessary, component (C) (hereinafter, these are referred to collectively as "emulsifiers").

The emulsification method is not particularly limited, and a known emulsification method such as a high-pressure emulsification method and a phase inversion emulsification method can be used.

The high-pressure emulsification method is a method in which the component (a) is in a liquid state, and then, the component (a) is preliminarily mixed with the emulsifier and water, and after the microemulsion is performed using a high-pressure emulsifier, the solvent is removed as needed. The method of bringing the component (A) into a liquid state may be heating only, heating after dissolving in a solvent, or heating after mixing with a nonvolatile substance such as a plasticizer. Examples of the solvent include organic solvents capable of dissolving the component (a), such as toluene, xylene, methylcyclohexane, and ethyl acetate.

The phase inversion emulsification method is a method in which the component (A) is heated and melted, and then a surfactant/water is added while stirring to form a W/O emulsion, and then the W/O emulsion is converted into an O/W emulsion by adding water, changing the temperature, or the like.

[ physical Properties and uses of Water-dispersible composition for fiber processing ]

The physical properties of the water-dispersible composition for fiber processing of the present invention are not particularly limited. The solid content concentration of the water-dispersible composition for fiber processing is not particularly limited, and it is usually used after appropriately adjusting the solid content to about 10 to 65 mass%. The volume average particle diameter of the water-dispersible composition for fiber processing is usually about 0.1 to 2 μm, and most of the particles are uniformly dispersed as particles of 1 μm or less, but from the viewpoint of storage stability, it is preferably 0.7 μm or less. The water-dispersible composition for fiber processing has a white to milky appearance, a pH of about 2 to 10, and a viscosity of about 10 to 1000 mPas (25 ℃, solid content concentration 50%).

The water-dispersible composition for fiber processing of the present invention can be used in combination with various fiber processing agents in various processes for fibers, thereby obtaining fibers excellent in slippage, hand feeling, and chalk mark resistance. The fiber processing agent is not particularly limited, and is preferably a water repellent agent or a stain resistance-imparting agent.

The amount of the water-dispersible composition for fiber processing of the present invention is not particularly limited, and is preferably about 1 to 20 mass%, more preferably about 1 to 10 mass% with respect to 100 mass% of the fiber processing agent. When the amount is 1 mass% or more, the slip property of the fiber becomes more excellent. Further, when the amount is 20 mass% or less, the fiber is more excellent in hand feeling and chalk mark resistance, and when a water repellent or a stain resistance-imparting agent is used, the functions of water repellency and stain resistance are further maintained, so that it is preferable.

The water repellent and the stain resistance-imparting agent are not particularly limited, and various known materials can be used. Hereinafter, the water repellent, stain resistance imparting agent and fiber will be described.

< Water repellent >

The water repellent agent is not particularly limited, but is preferably a non-fluorine-based water repellent agent in view of environment.

Examples of the non-fluorine-containing water repellent include compounds having a long-chain hydrocarbon group in the molecule. The compound having a long-chain hydrocarbon group in the molecule is not particularly limited, but is preferably a (meth) acrylate polymer obtained by reacting a monomer containing a long-chain hydrocarbon group-containing (meth) acrylate. The long-chain hydrocarbon group is preferably an alkyl group or alkenyl group having 12 to 24 carbon atoms, in view of excellent water repellency. The alkyl group and the alkenyl group may be linear or branched. Examples of the monomer other than the long-chain hydrocarbon group-containing (meth) acrylate include (meth) acrylates other than long-chain hydrocarbon group-containing (meth) acrylates, (meth) acrylamides, (meth) acrylic acids, (meth) acrylonitriles, styrenes, α, β -unsaturated dicarboxylic acids (anhydrides), and the like.

Examples of the long-chain hydrocarbon group-containing (meth) acrylate include lauryl (meth) acrylate, tridecyl (meth) acrylate, tetradecyl (meth) acrylate, pentadecyl (meth) acrylate, palmityl (meth) acrylate, heptadecyl (meth) acrylate, stearyl (meth) acrylate, nonadecyl (meth) acrylate, eicosyl (meth) acrylate, heneicosyl (meth) acrylate, docosyl (meth) acrylate, tricosyl (meth) acrylate, tetracosyl (meth) acrylate, isododecyl (meth) acrylate, isotridecyl (meth) acrylate, isotetradecyl (meth) acrylate, isopentadecyl (meth) acrylate, isohexadecyl (meth) acrylate, and mixtures thereof, Isoheptadecyl (meth) acrylate, isostearyl (meth) acrylate, and the like.

Examples of commercially available products of the non-fluorine-based water repellent agent include "ネオシード (trade name: NeoSeed)" (registered trademark) NR-90 (manufactured by Rihua chemical Co., Ltd.), NR-158 (manufactured by Rihua chemical Co., Ltd.), TH-44 (manufactured by Rihua chemical Co., Ltd.), パラジン HC86 (manufactured by Kyowa Kagaku K.K.), パラジン HC200 (manufactured by Kyowa Kagaku K.K.), PW-182 (manufactured by Dahua chemical Co., Ltd.), "フォボール (trade name: PHOBOOL)" (registered trademark) RSH (manufactured by Henshimai Kagaku K.K. (ハンツマン. ジャパン strain), "PARAGIUM" (trade name: PARAGIUM) "(registered trademark) ECO-500 (manufactured by Dayu chemical Co., Ltd.) (Nakayasu パラヂウム chemical Co., Ltd.), N018X (nano ナノテックス strain), ZERAN R-3 (manufactured by Hensmei Japan K.K.) and PM-3705 (manufactured by 3M corporation (スリーエム)), and the like.

< stain resistance-imparting agent >

The stain-proofing agent is not particularly limited. The stain-proofing agent includes, for example, a non-fluorine-based compound, and specifically, a silicone-based compound.

Examples of the silicone compound include ゲラネックス SH (English name: Geranex SH) (Songbi oil & fat pharmaceutical Co., Ltd.), ドライポン 600E (English name: DRYPON 600E) (manufactured by Niwawa chemical Co., Ltd.), リケンパラン SG-54 (English name: RIKEN PALAN SG-54) (Sanmarie chemical Co., Ltd.), ライトシリコーン (English name: Light silicone) P-290E (North Guanghi ケミカル (Ltd.)), ポロン MR (English name: POLON MR) (shin-Etsu chemical industry Co., Ltd.), POLON MF-49 (shin-Etsu chemical industry Co., Ltd.), ネオシード (English name: oSeeed) NR8000 (Niwawa chemical Co., Ltd.), KF-96 series (shin-Etsu chemical industry Co., Ltd.), 8005 (shin-chemical industry Co., Ltd.), and KF-8005 (shin-chemical industry Co., Ltd.), SF-8417 (Torredo Kangning Co., Ltd. (Torredo レ & ダウコーニング (Ltd.))), MQ-1600 (Torredo Kangning Co., Ltd.), and the like.

< fiber >

The fibers may be natural fibers or chemical fibers. Examples of natural fibers include plant fibers such as cotton, hemp, flax, coconut, rush and the like; animal fibers such as wool, goat wool, mohair, cashmere, camel hair, silk, etc.; mineral fibers such as asbestos. Examples of the chemical fibers include inorganic fibers such as rock fibers, metal fibers, graphite, silica, and titanate; regenerated cellulose fibers such as rayon, cuprammonium fibers, viscose fibers, Polynosic (Polynosic) fibers, and refined cellulose fibers; melt spinning cellulose fibers; protein fibers such as milk protein and soybean protein; regenerated/semi-synthetic fibers such as regenerated silk and alginic acid fiber; synthetic fibers such as polyamide fibers, polyester fibers, cationic dyeable polyester fibers, polyethylene fibers, polypropylene fibers, polyurethane fibers, acrylic fibers, polyethylene fibers, polyvinylidene fibers, polystyrene fibers, and the like. Two or more of these fibers may be combined (blended, mixed, interwoven, etc.).

The polyester fiber includes a fiber composed of a polymer obtained by polycondensation through a reaction of forming an ester bond, such as a polylactic acid (PLA) fiber including a polyethylene terephthalate (PET) fiber, a polytrimethylene terephthalate (PTT) fiber, a polybutylene terephthalate (PBT) fiber, a polytrimethylene terephthalate (PPT) fiber, a polyethylene naphthalate (PEN) fiber, or a polyarylate fiber. Examples of the fibers to be combined with the polyester fibers include synthetic fibers such as cellulose fibers, polyamide fibers, and polyurethane fibers, and natural fibers.

The polyamide fiber is a fiber which is essentially composed of polyamide and can be formed into a composite, and examples thereof include nylon 6, nylon 66, nylon 610, nylon 11, nylon 4, nylon 7, and aromatic nylon (aromatic polyamide). Polyamides are generally obtained by polycondensation of the reaction forming amide bonds.

Examples of the form of the fiber include woven fabric, knitted fabric, cloth, thread, cheese (cheese), skein (skein), and nonwoven fabric.

The water-dispersible composition for fiber processing of the present invention is preferably used for polyester fibers, polyamide fibers, and cotton. In particular, polyester fiber and cotton are preferable.

< fiber processing >

The method of processing the fibers using the water-dispersible composition for fiber processing of the present invention and the fiber processing agent is not particularly limited, and examples thereof include processing methods such as dipping, spraying, and coating, and processing methods such as cleaning methods. In addition, it is preferable that the water-dispersible composition for fiber processing and the fiber processing agent are attached to fibers and then dried to remove water.

In the above processing, the total amount of the water-dispersible composition for fiber processing and the fiber processing agent adhering to the fiber can be appropriately adjusted depending on the degree of the desired function, but is preferably adjusted to 0.1 to 10% by mass, more preferably 0.5 to 2% by mass, in terms of solid content, relative to the fiber. When the total amount of the above-mentioned adhesion is less than 0.1 mass%, the effect is hardly exhibited, and when it exceeds 10 mass%, the cost efficiency becomes low.

It is preferable to suitably perform heat treatment after processing the fiber using the water-dispersible composition for fiber processing of the present invention and the above-mentioned fiber processing agent. The temperature condition is not particularly limited, but is usually about 110 to 180 ℃.

As applications of the fibers subjected to the above processing, examples of objects to which water repellency and soil resistance are imparted include clothes such as coats, uniforms, and sportswear; sanitary materials such as masks, gauzes, paper diapers and the like; vehicle interior materials for automobiles, airplanes, railways, ships, and the like; bedding articles such as quilts, mattresses, sheets, pillows, quilt covers, blankets, toweling quilts and the like; indoor ornaments such as curtains, shutters, sofas, chairs, cushions, wallpaper, carpets, felts, tablecloths, back cushions, partition fans and the like; industrial materials such as stage curtains, black curtains, tarpaulins for engineering, tents, filters, and the like.

The fiber subjected to the above processing is particularly suitable for use in clothing or bedding called a jacket, specifically, fiber products such as clothing articles and non-clothing articles such as a down clothing, a coat, a jacket, a wind coat, a blouse, a dress shirt, a skirt, pants, gloves, a hat, a coverall, a quilt drying cover, a curtain, a tent and the like, because the fiber has various functions such as excellent water repellency, washing durability, stain resistance and the like, and has a soft hand feeling.

Examples

The present invention will be described in more detail below by way of examples of the present invention, but the present invention is not limited to these examples. In the examples, "part" and "%" represent "part by mass" and "% by mass", respectively.

< production of rosin-based resin (A) >

Production example 1

Into a reaction vessel equipped with a stirrer, a condenser, a thermometer, and a nitrogen inlet/steam inlet, 100 parts of disproportionated rosin (trade name: ロンヂス R (RONDIS R), available from seikagawa chemical industries co., ltd., acid value 160, softening point 70 c) and 3 parts of fumaric acid were charged, reacted at 220 c for 2 hours under a nitrogen gas stream, 10.7 parts of pentaerythritol and 1.5 parts of glycerin were charged, reacted at 250 c for 2 hours under a nitrogen gas stream, and then further heated to 280 c and reacted at the same temperature for 12 hours, thereby completing esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (a1) (hereinafter referred to as (a1) component).

Production example 2

In a reaction vessel similar to that of example 1, 100 parts of gum rosin (acid value: 190mgKOH/g, softening point: 80 ℃) produced in Indonesia from southern pine and 12.4 parts of pentaerythritol were charged, and then reacted at 250 ℃ for 2 hours under a nitrogen stream, followed by further heating to 280 ℃ and reacting at the same temperature for 12 hours, thereby completing esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (a2) (hereinafter referred to as (a2) component).

Production example 3

Into the same reaction vessel as in example 1, 100 parts of disproportionated rosin (trade name "ロンヂス R (RONDIS R)", manufactured by Mitsukawa chemical industries, Ltd., acid value 160, softening point 70 ℃ C.) and 11.6 parts of glycerin were charged, reacted at 250 ℃ for 2 hours under a nitrogen gas flow, and then further heated to 280 ℃ and reacted at the same temperature for 12 hours, thereby completing esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (A3) (hereinafter referred to as (A3) component).

Production example 4

100 parts of gum rosin (CG-WW) produced in China and 1 part of fumaric acid were charged into the same reaction vessel as in example 1, reacted at 220 ℃ for 2 hours under a nitrogen stream, 12.7 parts of pentaerythritol was charged and reacted at 250 ℃ for 2 hours, and then the temperature was further raised to 280 ℃ and reacted at the same temperature for 12 hours, thereby completing esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (a4) (hereinafter referred to as (a4) component).

Production example 5

100 parts of polymerized rosin (trade name: アラダイム R-140 (AraYME R-140, manufactured by Mitsukawa chemical industries, Ltd.), 11.7 parts of pentaerythritol and 0.6 part of glycerin were charged into the same reaction vessel as in example 1, reacted at 250 ℃ for 2 hours under a nitrogen gas flow, and then further heated to 280 ℃ and reacted at the same temperature for 12 hours to complete esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (a5) (hereinafter referred to as (a5) component).

Production example 6

Into the same reaction vessel as that of example 1, 50 parts of polymerized rosin (trade name: アラダイム R-140 (AraYME R-140), manufactured by Mitsuwa chemical industries, Ltd., acid value 140, softening point 140 ℃ C.) and CG-WW50 parts were charged, 11.1 parts of pentaerythritol and 0.5 part of glycerin were charged, and after reaction at 250 ℃ for 2 hours under a nitrogen gas stream, the temperature was further raised to 280 ℃ and the reaction was carried out at the same temperature for 12 hours, thereby completing esterification. Thereafter, the inside of the reaction vessel was depressurized to remove water and the like, thereby obtaining a rosin-based resin (a6) (hereinafter referred to as (a6) component).

The softening point (Sp (. degree. C.)) of the rosin-based resin in each production example was measured by the ring and ball method according to JIS K5902. The results are shown in Table 1.

The acid value and the hydroxyl value of the rosin-based resin in each production example were measured in accordance with JIS K0070. The results are shown in Table 1.

(measurement of weight average molecular weight (Mw))

The weight average molecular weight (Mw) of the rosin-based resins of production examples 1 to 6 was calculated from polystyrene conversion values obtained from calibration curves of standard polystyrene by a Gel Permeation Chromatography (GPC) method. The results are shown in Table 1. The GPC method is measured under the following conditions.

An analysis device: HLC-8320 (manufactured by Tosoh corporation).

A chromatographic column: TSKgelSuperHM-Lx 3 roots.

Eluent: tetrahydrofuran.

Concentration of injected sample: 5 mg/mL.

Flow rate: 0.6 mL/min.

Injection amount: 40 μ L.

Temperature of the column: at 40 ℃.

A detector: and RI.

TABLE 1

[ preparation of Water-dispersible composition for fiber processing ]

Example 1

100 parts of the component (A1) of production example 1 was dissolved in 70 parts of toluene at 80 ℃ for 3 hours, and then 10 parts of EMALEX630 (nonionic surfactant, HLB15, manufactured by Nippon emulsion Co., Ltd. (Nippon エマルジョン (Ltd)) and 140 parts of water were added in terms of solid content and stirred for 1 hour. Then, high-pressure emulsification was performed under a pressure condition of 30MPa using a high-pressure emulsifier (manufactured by mantongolian corporation (マントンガウリン)) to obtain an emulsion. Then, at 70 ℃ 2.93X 10^-2The mixture was distilled under reduced pressure under MPa for 6 hours to obtain a water-dispersible composition for fiber processing having a solid content of 30%.

Example 2

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1, except that the component (a1) was replaced with the component (a2) of production example 2.

Example 3

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1, except that the component (a1) was replaced with the component (A3) of production example 3.

Example 4

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1, except that the component (a1) was replaced with the component (a4) of production example 4.

Example 5

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1, except that the component (a1) was replaced with the component (a5) of production example 5.

Example 6

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1, except that the component (a1) was replaced with the component (a6) of production example 6.

Example 7

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1 except that the component (A1) was replaced with a hydrogenated rosin ester (trade name "KE-359", manufactured by Seikaga chemical industries, Ltd.) (hereinafter referred to as component (A7)). The component (A7) had a softening point of 95 ℃, an acid value of 15mgKOH/g, a hydroxyl value of 44mgKOH/g, a weight average molecular weight (Mw) of 1231, and a color tone of 50 Hansen.

Example 8

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1 except that the EMALEX630 was replaced with EMULGEN220(エマルゲン 220) (nonionic surfactant, HLB14.2, manufactured by kao chemical corporation, kao ケミカル).

Example 9

A water-dispersible composition for fiber processing was obtained in the same manner as in example 5 except that the EMALEX630 was replaced with EMULGEN220 (nonionic surfactant, HLB14.2, manufactured by kaowang chemical company).

Example 10

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1 except that the EMALEX630 was replaced with NOIGEN XL-61(ノイゲン XL-61) (nonionic surfactant, HLB12.5, manufactured by first Industrial pharmaceutical Co., Ltd.).

Example 11

A water-dispersible composition for fiber processing was obtained in the same manner as in example 1 except that the EMALEX630 was replaced with EMULGEN103 (nonionic surfactant, HLB8.1, manufactured by kaowang chemical company).

Comparative example 1

The same procedure was carried out except for using 5 parts of CATIOGEN TMP (カチオーゲン TMP) (cationic surfactant, manufactured by first industrial pharmaceutical company) instead of EMALEX630 in example 5, to obtain a water-dispersed composition for fiber processing.

(emulsion stability)

In each of examples and comparative examples, the quality of handling (foaming or generation of aggregates) when each rosin resin was emulsified was visually observed and evaluated according to the following criteria, and the results are collectively shown in table 2. In the case of a slightly good characteristic, a "+" is added to the following reference, and in the case of a slightly poor characteristic, a "-" is added to the reference.

Very good: hardly foams or generates aggregates, and is excellent in workability.

O: little foaming or aggregate generation and good operability.

And (delta): slightly more foaming or aggregate formation was observed, and the workability was slightly poor.

X: much foaming or aggregate formation was observed, and the workability was poor.

TABLE 2

[ preparation of non-fluorine-based Water repellent composition ]

Evaluation example 1

95 parts of PM-3705 (manufactured by 3M) as a non-fluorine-based water repellent agent was mixed with 5 parts (in terms of solid content) of the water-dispersed composition for fiber processing of example 1, and further diluted with water to prepare a non-fluorine-based water repellent composition having a solid content of 5 mass%.

Evaluation example 2

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1 except that the water-dispersed composition for fiber processing of example 2 was used as the water-dispersed composition for fiber processing.

Evaluation example 3

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 3 was used as the water-dispersed composition for fiber processing.

Evaluation example 4

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 4 was used as the water-dispersed composition for fiber processing.

Evaluation example 5

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 5 was used as the water-dispersed composition for fiber processing.

Evaluation example 6

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 6 was used as the water-dispersed composition for fiber processing.

Evaluation example 7

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 7 was used as the water-dispersed composition for fiber processing.

Evaluation example 8

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 8 was used as the water-dispersed composition for fiber processing.

Evaluation example 9

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 9 was used as the water-dispersed composition for fiber processing.

Evaluation example 10

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 10 was used as the water-dispersed composition for fiber processing.

Evaluation example 11

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1, except that the water-dispersed composition for fiber processing of example 11 was used as the water-dispersed composition for fiber processing.

Comparative evaluation example 1

A non-fluorine-based water repellent composition was obtained in the same manner as in evaluation example 1 except that the water-dispersed composition for fiber processing of comparative example 1 was used.

(preparation of test piece)

< evaluation of Water repellency >

In the non-fluorine-based water repellent composition obtained in evaluation example 1, a polyester fabric was impregnated and pressed using a mangle. Thereafter, the polyester fabric to which the above composition was attached was dried at 120 ℃ for 2 minutes using a pin tenter, thereby obtaining water repellent processed fibers (test piece of polyester fabric).

(evaluation examples 2 to 11 and comparative evaluation example 1)

Water-repellent processed fibers were produced in the same manner as in evaluation example 1, except that the type of the water-dispersible composition for fiber processing in evaluation example 1 was changed as shown in table 3.

(Water repellency: spray test)

The water repellency of the water-repellent processed fiber was evaluated by a spraying method according to JIS-L-1092 (AATCC-22). The results are shown in Table 3. The water repellency is represented by a water repellency number as described below, and a larger score indicates better water repellency. The results were evaluated visually on the following scale.

Water repellency: status of state

5: the surface was not in a wet state.

4: the surface shows a slightly wet-adhered state.

3: the surface shows a partially wet condition.

2: showing a wet state on the surface.

1: the surface as a whole shows a wet state.

0: both the front and back sides show a completely wet state.

(test for washing durability and Water repellency)

The water repellent processed fiber was washed 10 times (HL10) in a washing liquid at 40 ℃ in accordance with JIS L-0217103, and then dried in a drum (30 minutes at 60 ℃) to obtain a fiber as a test piece for evaluating washing durability, and washing durability and water repellency was evaluated in the same manner as the above-mentioned spray test. The results are shown in Table 3.

(slippage test)

The water-repellent processed fibers were tested by slipping the warp under a load of 117.2N (12kgw) in accordance with JIS L1096-99.8.21.1 seam slipping method B, and the seam slipping property was evaluated by measuring the slipping resistance. The results are shown in Table 3. The smaller the value, the more excellent the seam slippage property is shown.

(hand feeling test)

The hand feel of the water-repellent processed fiber was evaluated in the following 5 stages. Evaluation was performed by 5 testers, and the average value was calculated. The results are shown in Table 3.

1: is very hard.

2: hard.

3: is slightly harder.

4: is soft.

5: is very soft.

(Chalk mark test)

After drawing a pattern on the water-repellent fiber by pressing a plastic rod having a tip diameter of 5mm, whether the pattern remained on the cloth was visually observed (so-called chalk mark test), and the chalk mark resistance was evaluated in 5 stages as follows. The results are shown in Table 3.

1: clear traces were found.

2: traces were found.

3: traces were found slightly.

4: almost no trace was found.

5: there were no traces at all.

TABLE 3

[ preparation of non-fluorine-based antifouling composition ]

Evaluation example 12

95 parts of Geranex SH (manufactured by Songbo oil & fat pharmaceuticals Co., Ltd.) as a non-fluorine-based stain-proofing agent was mixed with 5 parts (in terms of solid content) of the fiber-processing water-dispersible composition of example 1, and the mixture was further diluted with water to prepare a non-fluorine-based stain-proofing agent composition having a solid content of 5 mass%.

Evaluation example 13

A non-fluorine-based antifouling agent composition was obtained in the same manner as in evaluation example 12, except that the water-dispersed fiber composition of example 2 was used as the water-dispersed fiber composition.

Evaluation example 14

A non-fluorine-based antifouling agent composition was obtained in the same manner as in evaluation example 12, except that the water-dispersed fiber composition of example 3 was used as the water-dispersed fiber composition.

Evaluation example 15

A non-fluorine-based antifouling agent composition was obtained in the same manner as in evaluation example 12, except that the water-dispersed fiber composition of example 7 was used as the water-dispersed fiber composition.

Comparative evaluation example 2

A non-fluorine-based antifouling agent composition was obtained in the same manner as in evaluation example 12, except that the water-dispersed fiber composition of comparative example 1 was used as the water-dispersed fiber composition.

(preparation of test piece)

< evaluation of antifouling Property >

In the non-fluorine type stain resistant agent composition obtained in evaluation example 12, a polyester fabric was impregnated and pressed using a mangle. Thereafter, the polyester fabric to which the treatment liquid was attached was dried at 120 ℃ for 2 minutes using a pin tenter, thereby obtaining a soil repellent fiber (polyester fabric test piece).

(evaluation examples 13 to 15 and comparative evaluation example 2)

Except that the type of the water-dispersible composition for fiber processing in evaluation example 12 was changed to that shown in table 4, the fibers for soil resistance processing were produced and evaluated in the same manner as in evaluation example 12. The results are shown in Table 4.

(stain resistance (SG Property): liquid stain test)

According to JIS-L-1919B method (spraying method), 100ml of a stain component (a 1: 1 mixed solution of edible red No. 2 0.1% and sucrose 10.0%) was dispersed on the above-mentioned anti-fouling fiber (20 cm. times.20 cm), and the fouling substance was adsorbed by using a filter paper having a diameter of 11 cm. After leaving for about 1 minute, the film was dried at room temperature to evaluate the stain-proofing property (SG property). The results were evaluated visually on the following scale. The results are shown in Table 4.

Degree of difficult contamination: status of state

5: no adhesion on the surface.

4: a slightly adherent state is shown on the surface.

3: the surface shows the state of partial attachment.

2: showing the state of adhesion on the surface.

1: the surface as a whole shows the state of adhesion.

0: both the front and back surfaces show a completely wetted state.

(test of washing durability and stain-proofing property (SG Property))

The liquid stain resistance evaluation was carried out in the same manner as in the above liquid stain evaluation except that the fibers obtained by subjecting the above fibers to 10 washing treatments in accordance with JIS-L-0217103 were used as test pieces for evaluating the washing durability, and the washing durability stain resistance (washing durability SG property) was evaluated. The results are shown in Table 4.

(slippage test)

The anti-soil processed fiber was tested by slipping the warp under a load of 117.2N (12kgw) according to JIS L1096-99.8.21.1 seam slipping method B, and the seam slipping property was evaluated. The results are shown in Table 4.

(hand feeling test)

The hand feel of the antifouling fibers was evaluated in the following 5 stages from the hand feel. Evaluation was performed by 5 testers, and the average value was calculated. The results are shown in Table 4.

1: is very hard.

2: hard.

3: is slightly harder.

4: is soft.

5: is very soft.

TABLE 4

Claims

1. A water-dispersible composition for fiber processing, wherein,

the resin composition contains a rosin resin as a component (A) and a nonionic surfactant as a component (B).

2. The fiber-processing water-dispersion composition according to claim 1,

the softening point of the rosin resin as the component (A) is 80 to 180 ℃.

3. The water-dispersible composition for fiber processing according to claim 1 or 2,

the rosin resin as the component (A) is a rosin ester.

4. The water-dispersible composition for fiber processing according to any one of claims 1 to 3,

the HLB of the nonionic surfactant as the component (B) is 7 to 19.

5. The water-dispersible composition for fiber processing according to any one of claims 1 to 4,

it is used for polyester fibers.

6. The water-dispersible composition for fiber processing according to any one of claims 1 to 4,

it is used for polyamide fibers.

7. The water-dispersible composition for fiber processing according to any one of claims 1 to 4,

it is used for cotton.